Method for determining rifamycin S by means of liquid chromatography
A technology of rifamycin and liquid chromatography, applied in the field of raw material rifamycin S after the cyclization reaction, can solve the problems of inability to obtain reaction data, quantitative precision deviation, etc.
Active Publication Date: 2020-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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[0005] At present, the first step reaction is mainly monitored by thin-layer chromatography. Although it can quickly detect whether the reactant is completely reacted, its quantitative precision deviation makes it impossible to obtain exact reaction data, so it cannot serve the production process well. improvement of
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Embodiment 1
[0035] Using rifamycin S as a raw material, the reaction equation and related substance structural formulas of benzoxazine rifamycin obtained through cyclization reaction are as follows:
[0036]
[0037] A 0.40M rifamycin S solution and a 1.36M dimethylol tert-butylamine solution were prepared with DMF as a solvent, and both flows were pumped into the reactor at 0.3mL / min for cyclization reaction to obtain rifamycin S-containing The product of the cyclization reaction.
[0038] Step 1. Prepare standard solution
[0039] Accurately weigh 125mg of rifamycin S standard substance, accurate to ±0.0001g, first dissolve it with acetonitrile and dilute to 10mL with buffer solution, then take 0.4mL, 0.8mL, 1.2mL, 1.6mL and 2mL solutions respectively, and set In a 25mL volumetric flask, add 1.6mL, 1.2mL, 0.8mL, 0.4mL and 0mL of acetonitrile respectively, and then dilute to 25mL, to obtain standard solutions with different concentration gradients, the concentrations were 0.27mmol / L...
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Abstract
The invention relates to a method for quantitatively analyzing a synthetic raw material rifamycin S of rifampicin by means of liquid chromatography. The method belongs to the field of chemical analysis, and comprises the steps of: 1, preparing a standard solution of a rifamycin S standard substance by using a buffer solution; 2, treating a cyclization reaction liquid, wherein the treatment is implemented by adding a crude product into an acetic acid solution, carrying out suction filtration to obtain a solid product containing rifamycin S, adding the solid product into acetonitrile for dissolving, fixing the volume of the solution by using a buffer solution, and filtering the solution by using a microporous filter membrane to remove impurities, thereby acquiring a liquid chromatography detection sample; 3, performing liquid chromatographic analysis on the standard solution, and drawing a standard curve; 4, and analyzing the sample by means of liquid chromatography, and comparing with the standard curve to determine the content of rifamycin S serving as a rifampicin synthetic raw material after cyclization reaction. According to the method, the content and a reaction conversion rateof the rifampicin synthetic raw material rifamycin S can be precisely determined, and the defects in the prior art are overcome.
Description
technical field [0001] The invention relates to a method for quantitatively analyzing rifampicin synthetic raw materials by using liquid chromatography, in particular to a method for measuring the raw material rifamycin S after the cyclization reaction in the rifampicin synthesis process by using liquid chromatography, belonging to field of chemical analysis. Background technique [0002] Rifampin (Rifampin) is a semi-synthetic broad-spectrum antibiotic belonging to the rifamycin class. It has a strong inhibitory and killing effect on tuberculosis. Lambert-positive bacteria are also effective. [0003] The synthesis of rifampicin in published patents generally includes two-step reactions, namely cyclization and condensation reactions. Chinese Invention Patent Application Publication No. 101486716A discloses the preparation method of high-quality rifampicin, using rifamycin S sodium salt to acidify with acetic acid to obtain free rifamycin S, and then reacting with dimethyl...
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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈光文温正慧韩梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI